The Rapid, At-Line Determination of Starch Content in Sucrose–Starch Blends Using Near-Infrared Reflectance Spectroscopy; A Process Analytical Technology Initiative

2005 ◽  
Vol 13 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Brad Swarbrick ◽  
Bronwyn Grout ◽  
James Noss
Keyword(s):  
Near Infrared ◽  
Process Analytical Technology ◽  
Starch Content ◽  
Spectroscopic Method ◽  
Laboratory Method ◽  
Content Uniformity ◽  
Testing Time ◽  
Near Infrared Reflectance ◽  
Starch Blends

A near infrared (NIR) reflectance spectroscopic method was developed for the rapid determination of starch content in the excipient material sucrose special powder, 4.6% starch. It was previously determined that the variability of starch content in individual bags within each delivery of this material was high. This required appropriate sample selection to provide a controlled content of starch before use in the pharmaceutical industry. Therefore, an NIR method was developed to reduce long laboratory testing time and to facilitate testing of the starch content of the material at-line in the receiving warehouse, [standard error of prediction ( SEP)NIR = 0.16% compared with 0.15% for the laboratory method]. Another important feature of the NIR starch model was its use as an at-line tool for in-house blending of sucrose–starch blends to determine blend homogeneity. In one particular application, a sucrose–starch blend, known to contain low starch levels, was spiked with commercially available starch and blended. The NIR method was used to make rapid decisions on content uniformity and the results obtained were in close agreement with laboratory assay data (mean starch content using the NIR method 4.5% compared with 4.6% for the laboratory method).

Comparison Between Liquid and Paste Karl Fischer Extractions for NIRS Water Calibrations

1989 ◽  
Vol 72 (2) ◽  
pp. 255-258 ◽  
Author(s):  
William R Windham
Keyword(s):  
Near Infrared ◽  
Starch Content ◽  
Water Concentration ◽  
Reference Method ◽  
Extraction Methods ◽  
Near Infrared Reflectance ◽  
Karl Fischer ◽  
Extraction Procedures ◽  
Primary Reference

Abstract The acceptance of near infrared reflectance spectroscopy (NIRS) for the routine analysis of water in forage was made possible by the application of Karl Fischer (KF) water analysis as the primary reference method during calibration. Water is extracted by ball milling the sample in the presence of methanol (1:50), and an aliquot of the liquid phase is sampled and titrated. An alternative extraction utilizes a 20 g sample with 20 mL methanol, and an aliquot of the paste is sampled and titrated. The objectives of this study were to compare extraction procedures (i.e., liquid vs paste) on the determination of water in 75 milled grains and concentrate rations, and to develop and compare NIRS calibrations for water on the basis of both extraction methods. The majority of the samples (N = 61) had a 1.05 percentage unit greater water content (P < 0.05) from the paste method than from the liquid method. Bias between the extraction procedures was positively correlated (r2 = 0.84) to starch content. The lowered extraction efficiency of the liquid method is explained by its inability to account for water bound to starch. NIRS calibration and equation validation statistics were superior with water data from the paste method. The increased calibration errors with the liquid method also appear to reflect the inability of the method to accurately measure the total water concentration of the samples in relation to the water measurement based on the NIRS signals. The study concludes that the KF paste method is a superior primary reference method for the determination of water in flour obtained from cereal grains and concentrate rations.

Development of an In-Line Near-Infrared Method for Blend Content Uniformity Assessment in a Tablet Feed Frame

2019 ◽  
Vol 73 (9) ◽  
pp. 1028-1040
Author(s):  
Yi Li ◽  
Carl A. Anderson ◽  
James K. Drennen ◽  
Christian Airiau ◽  
Benoît Igne
Keyword(s):  
Sample Size ◽  
Near Infrared ◽  
Process Analytical Technology ◽  
Spectroscopic Method ◽  
Integration Time ◽  
Effective Sample Size ◽  
Content Uniformity ◽  
Representative Sampling ◽  
Factors Affecting ◽  
The Impact

Process analytical technology (PAT) has shown great potential for in-line tableting process monitoring. The study focuses on the development and validation of an in-line near-infrared (NIR) spectroscopic method for the determination of content uniformity of blends in a tablet feed frame. An in-line NIR method was developed after careful evaluation of the impact of potential experimental factors on the robustness and model accuracy and precision. The NIR method was validated according to the principles outlined in International Conference on Harmonization–Q2 for validation of analytical procedures and was demonstrated to be suitable for monitoring blend content for the formulation under evaluation. Reliable measurements of blend homogeneity rely on representative sampling. To reach the appropriate scale of scrutiny for a unit dose, the study assessed factors that influence the effective sample size measured by NIR. Spectral averaging, integration time, and feed frame paddle wheel speed were found to influence the effective sample size measured by the NIR probe. The effective sampling size was also estimated by comparing the distribution of predicted values with the reference values. The development of a robust, in-line PAT method was facilitated by thorough understanding of the sensitivity of PAT sensors to factors affecting pharmaceutical processes and products.

Determination of starch content in single kernel using near-infrared hyperspectral images from two sides of corn seeds

2020 ◽  
Vol 110 ◽  
pp. 103462
Author(s):  
Chen Liu ◽  
Wenqian Huang ◽  
Guiyan Yang ◽  
Qingyan Wang ◽  
Jiangbo Li ◽  
...  
Keyword(s):  
Near Infrared ◽  
Starch Content ◽  
Hyperspectral Images ◽  
Two Sides

Prediction of crude protein content in field peas using near infrared reflectance spectroscopy

2006 ◽  
Vol 86 (1) ◽  
pp. 157-159 ◽  
Author(s):  
G. C. Arganosa ◽  
T. D. Warkentin ◽  
V. J. Racz ◽  
S. Blade ◽  
C. Phillips ◽  
...  
Keyword(s):  
Crude Protein ◽  
Near Infrared ◽  
Spectroscopic Method ◽  
Correlation Coefficients ◽  
Reflectance Spectroscopy ◽  
Field Pea ◽  
Infrared Reflectance ◽  
Near Infrared Reflectance Spectroscopy ◽  
Near Infrared Reflectance ◽  
Infrared Reflectance Spectroscopy

A rapid, near-infrared spectroscopic method to predict the crude protein contents of 72 field pea lines grown in Saskatchewan, both whole seeds and ground samples, was established. Correlation coefficients between the laboratory and predicted values were 0.938 and 0.952 for whole seed and ground seed, respectively. Both methods developed are adequate to support our field pea breeding programme. Key words: Field pea, near-infrared reflectance spectroscopy, crude protein

scholarly journals Methods for predicting the energy value of pet foods

2009 ◽  
Vol 38 (spe) ◽  
pp. 1-14 ◽  
Author(s):  
Carlos Castrillo ◽  
Marta Hervera ◽  
Maria Dolores Baucells
Keyword(s):  
Near Infrared ◽  
Metabolizable Energy ◽  
Apparent Digestibility ◽  
Crude Fibre ◽  
Near Infrared Reflectance ◽  
Energy Value ◽  
Close Relationship ◽  
Accuracy Of Prediction

The energy value of foods as well as energy requirements of dogs and cats is currently expressed in terms of metabolizable energy (ME). The determination of ME content of foods requires experimental animals and is too expensive and time consuming to be used routinely. Consequently, different indirect methods have been proposed in order to estimate as reliably an accurately as possible the ME content of pet food. This work analyses the main approaches proposed to date to estimate the ME content of foods for cats and dogs. The former method proposed by the NRC estimates the ME content of pet foods from proximal chemical analysis using the modified Atwater factors, assuming constant apparent digestibility coefficients for each analytical fraction. Modified Atwater factors systematically underestimate the ME content of low-fibre foods whereas they overestimate those that are high in fibre. Recently, different equations have been proposed for dogs and cats based in the estimation of apparent digestibility of energy by the crude fibre content, which improve the accuracy of prediction. In any case, whatever the method of analysis used, differences in energy digestibility related with food processing and fibre digestibility are unlikely to be accounted for. A simple in vitro enzymatic method has been recently proposed based in the close relationship that exist between energy digestibility and organic matter disappearance after two consecutive enzymatic (pepsin-pancreatin) incubation of food sample. Nutrient composition and energy value of pet foods can be also accurately and simultaneously predicted using near infrared reflectance spectroscopy (NIRS).

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